CN102225331B - Particle electrode catalyst filling material for three-dimensional electrodes and preparation method thereof - Google Patents
Particle electrode catalyst filling material for three-dimensional electrodes and preparation method thereof Download PDFInfo
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- CN102225331B CN102225331B CN2011100839450A CN201110083945A CN102225331B CN 102225331 B CN102225331 B CN 102225331B CN 2011100839450 A CN2011100839450 A CN 2011100839450A CN 201110083945 A CN201110083945 A CN 201110083945A CN 102225331 B CN102225331 B CN 102225331B
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Abstract
The invention discloses a particle electrode catalyst filling material for three-dimensional electrodes, and a preparation method thereof. The particle electrode catalyst filling material comprises alumina particle electrodes and graphene-modified stannic oxide coated on the alumina particle electrodes. The preparation method of the particle electrode catalyst filling material comprises the following steps of 1) carrying out a pretreatment on alumina particle electrodes, 2) preparing graphene-stannic chloride sol, and 3) mixing the pretreated alumina particle electrodes and the graphene-stannic chloride sol, stirring uniformly the mixture by a constant temperature magnetic heating stirrer, standing, aging, then carrying out a centrifugal separation process, drying and calcining to obtain a particle electrode catalyst filling material for three-dimensional electrodes. The preparation method has the advantages of simple process, low preparation cost, and easy popularization and application. The particle electrode catalyst filling material prepared through the preparation method has the advantages of stable property, high electrocatalysis efficiency and difficult stratification.
Description
Technical field
The invention belongs to the electrochemical catalysis technical field, be specifically related to particle electrode catalyst filling of a kind of three-diemsnional electrode and preparation method thereof.
Background technology
Three-diemsnional electrode (Three-Dimensional Electrodes) is a kind of novel electrochemical reactor, is granule electrode or bed electrode again.It is granular or other clastic working electrode material of filling and make particle surface charged between the conventional two-dimensional electrolytic tank electrode, thereby makes electric charge with three-dimensional spatial distribution.The three-dimensional nature of electrode has increased the electrode reaction area on the one hand greatly, has improved electrode reaction speed, and the space-time yield that characterizes reaction yield is improved a lot than plate electrode; Owing to the existence of internal resistance, electrode potential and electric current are uneven distribution on whole three-diemsnional electrode body on the other hand.The sorting technique of three-dimensional electric degree is a lot, can be divided into unipolarity and multipole property by particle polarity; Can be divided into rectangle and cylindrical by electrode configuration; Can be divided into parallel type and vertical-type by electric current and flow direction relations; Can be divided into by particulate material filling state fixed form and suspended pattern are arranged.
At present PbO is arranged with the three dimensional particles electrode that is used for wastewater treatment
2, apply the SnO that mixes Sb on the titanium foam beads
2, Ebonex (a kind of pottery) goes up and applies RuO
2Or SnO
2Sb
2O
3, Pt and Ni are deposited on the Ebonex carrier, support SnO on the hydrocarbon black powder
2Sb, activated carbon supported CeO
2Sb
2O
3But above-mentioned granule electrode is unipolarity, is unfavorable for practical applications, and PbO
2In reaction, have a large amount of Pb strippings, be prone to cause secondary pollution.And be the Bipolar Micro-Electrode electrode with active carbon, mica, silica and the active carbon of filming, because the proportion of filler and particle diameter etc. are inconsistent, the easy layering of electrode material and insulating materials during actual motion, thus make the insulant inefficacy.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art; A kind of stable in properties is provided; Electro-catalysis efficient is high, is difficult for the particle electrode catalyst filling of the three-diemsnional electrode of layering, and the preparation method of this particle electrode catalyst filling also is provided.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is: a kind of particle electrode catalyst filling of three-diemsnional electrode; It is characterized in that this catalyst is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 9~12: 1, and the mass ratio of said Graphene and tin ash is 0.1~2.5: 1000.
The present invention also provides the preparation method of the particle electrode catalyst filling of this three-diemsnional electrode, it is characterized in that, this method may further comprise the steps:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 5~10, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 100 ℃~150 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: in 20mL~100mL mass concentration is 5%~40% butter of tin solution, add 0.5mg~15mg Graphene; Vibration evenly; Behind ultrasonic dispersion 20min~30min; Stir with constant temperature magnetic force heating stirrer; Speed by 20/min~30 droplet/min when stirring dropwise adds the ammoniacal liquor that concentration is 0.3mol/L~5mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 1~12 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind still aging then 10h~18h; The solid that centrifugation is obtained is to dry under 80 ℃~90 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 2h~4h under 400 ℃~600 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
The mass concentration of butter of tin solution is 20% described in the above-mentioned steps (2).
The concentration of ammoniacal liquor is 0.4mol/L described in the above-mentioned steps (2).
Roasting time is 2h described in the above-mentioned steps (3).
The present invention compared with prior art has the following advantages:
1, the particle electrode catalyst filling stable in properties of three-diemsnional electrode of the present invention, electro-catalysis efficient is high, is difficult for layering, and is reusable.
2, preparation method of the present invention is simple, and low cost of manufacture is easy to apply.
3, the present invention does not use strong oxidizer and reducing agent in the modification of Graphene, has farthest brought into play the advantage of Graphene, and is nontoxic to environment, can not cause secondary pollution.
4, adopt the particle electrode catalyst filling of the present invention's preparation to combine to obtain the three dimensional particles electrode with two-dimensional electrode, increased the response area of electrode greatly, improved electrode reaction speed.
Through embodiment, technical scheme of the present invention is done further detailed description below.
The specific embodiment
Embodiment 1
The particle electrode catalyst filling of the three-diemsnional electrode of present embodiment is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 9: 1, and the mass ratio of said Graphene and tin ash is 0.1: 1000.
Its preparation method is:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 5, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 100 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: to the 50mL tin concentration is to add the 0.5mg Graphene in 20% the butter of tin solution; Vibration evenly; Behind the ultrasonic dispersion 20min; Stir with constant temperature magnetic force heating stirrer; Speed by 20/min when stirring dropwise adds the ammoniacal liquor that concentration is 0.4mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 12 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind the still aging then 12h; The solid that centrifugation is obtained is to dry under 80 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 2h under 550 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
Embodiment 2
The particle electrode catalyst filling of the three-diemsnional electrode of present embodiment is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 12: 1, and the mass ratio of said Graphene and tin ash is 1: 1000.
Its preparation method is:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 8, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 120 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: to the 20mL tin concentration is to add the 1.2mg Graphene in 20% the butter of tin solution; Vibration evenly; Behind the ultrasonic dispersion 30min; Stir with constant temperature magnetic force heating stirrer; Speed by 20/min when stirring dropwise adds the ammoniacal liquor that concentration is 0.3mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 1 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind the still aging then 10h; The solid that centrifugation is obtained is to dry under 90 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 4h under 400 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
Embodiment 3
The particle electrode catalyst filling of the three-diemsnional electrode of present embodiment is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 10: 1, and the mass ratio of said Graphene and tin ash is 1.2: 1000.
Its preparation method is:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 10, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 150 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: to the 100mL tin concentration is to add the 2.2mg Graphene in 5% the butter of tin solution; Vibration evenly; Behind the ultrasonic dispersion 20min; Stir with constant temperature magnetic force heating stirrer; Speed by 25/min when stirring dropwise adds the ammoniacal liquor that concentration is 3mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 7 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind the still aging then 18h; The solid that centrifugation is obtained is to dry under 85 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 2h under 600 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
Embodiment 4
The particle electrode catalyst filling of the three-diemsnional electrode of present embodiment is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 11: 1, and the mass ratio of said Graphene and tin ash is 2.5: 1000.
Its preparation method is:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 7, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 130 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: to the 20mL tin concentration is to add the 5.0mg Graphene in 40% the butter of tin solution; Vibration evenly; Behind the ultrasonic dispersion 25min; Stir with constant temperature magnetic force heating stirrer; Speed by 30/min when stirring dropwise adds the ammoniacal liquor that concentration is 5mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 6 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind the still aging then 18h; The solid that centrifugation is obtained is to dry under 80 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 3h under 500 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
Embodiment 5
The particle electrode catalyst filling of the three-diemsnional electrode of present embodiment is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 10: 1, and the mass ratio of said Graphene and tin ash is 1.5: 1000.
Its preparation method is:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 7, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 120 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: to the 20mL tin concentration is to add the 10mg Graphene in 40% the butter of tin solution; Vibration evenly; Behind the ultrasonic dispersion 20min; Stir with constant temperature magnetic force heating stirrer; Speed by 30/min when stirring dropwise adds the ammoniacal liquor that concentration is 4mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 10 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind the still aging then 15h; The solid that centrifugation is obtained is to dry under 90 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 3h under 550 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
Embodiment 6
The particle electrode catalyst filling of the three-diemsnional electrode of present embodiment is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 9: 1, and the mass ratio of said Graphene and tin ash is 2: 1000.
Its preparation method is:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 10, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 150 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: to the 60mL tin concentration is to add the 15mg Graphene in 20% the butter of tin solution; Vibration evenly; Behind the ultrasonic dispersion 25min; Stir with constant temperature magnetic force heating stirrer; Speed by 25/min when stirring dropwise adds the ammoniacal liquor that concentration is 2mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 8 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind the still aging then 16h; The solid that centrifugation is obtained is to dry under 85 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 4h under 450 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
Embodiment 7
The electrolysis effectiveness test of tin ash-aluminium oxide particles that the particle electrode catalyst filling of three-diemsnional electrode of the present invention-Graphene is modified:
With the inert metal titanium as working electrode; Be combined into the three dimensional particles electrode with the particle electrode catalyst filling of embodiment of the invention 1-6 preparation; To volumetric concentration is that the eosin solution of 50mg/L carries out degradation treatment; It is the eosin solution of 50mg/L that electrode is placed 20mL concentration, under the 16.0v voltage conditions, measures the degradation rate of eosin behind the degraded 1h.Its result sees the following form.
The electrolysis effectiveness of the particle electrode catalyst filling for preparing in table 1 embodiment of the invention detects
Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
Degradation rate (%) | 79.67 | 78.95 | 78.51 | 75.46 | 82.47 | 77.21 |
As working electrode, be combined into three dimensional particles electrode with tin ash-aluminium oxide particles with the inert metal titanium, use the same method eosin solution is carried out degradation treatment, the eosin degradation rate is merely 61.20% behind the degraded 1h.This shows that the particle electrode catalyst filling electro-catalysis efficient of the three-diemsnional electrode of the present invention's preparation is high.
Embodiment 8
The stability test of tin ash-aluminium oxide particles that the particle electrode catalyst filling of three-diemsnional electrode-Graphene is modified:
As working electrode, the particle electrode catalyst filling for preparing with 1g embodiment 3 is combined into three-diemsnional electrode with the inert metal titanium, and it is the phenol solution of 50mg/L that three-diemsnional electrode is placed 200mL concentration; Under the 10.05V voltage conditions, behind the degraded 1h, solution centrifugal is separated; After the solid oven dry after separating; With distilled water washing, dipping, behind the repeated washing, oven dry three times, carry out electro-catalysis degraded test under the same conditions.Repeat five times continuously, record the phenol degrading rate and be followed successively by: 65.71%, 62.43%, 60.53%, 59.69%, 58.31%.This shows that the particle electrode catalyst filling stability of the present invention's preparation is higher, reusable.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalent structure that above embodiment did according to the present invention, all still belongs in the protection domain of technical scheme of the present invention.
Claims (4)
1. the particle electrode catalyst filling of a three-diemsnional electrode is characterized in that, this particle electrode catalyst filling is made up of aluminium oxide particles electrode and the tin ash that the Graphene that is carried on the aluminium oxide particles electrode is modified; The mass ratio of the tin ash that said aluminium oxide particles electrode and Graphene are modified is 9~12: 1, and the mass ratio of said Graphene and tin ash is 0.1~2.5: 1000;
The preparation method may further comprise the steps:
(1) preliminary treatment of aluminium oxide particles electrode: the mass ratio by aluminium oxide particles electrode and distilled water is 1: 5~10, with the aluminium oxide particles electrode with distilled water immersion, washing three times after, in temperature is 100 ℃~150 ℃ baking oven, dry;
(2) preparation of Graphene-butter of tin colloidal sol: in 20mL~100mL mass concentration is 5%~40% butter of tin solution, add 0.5mg~15mg Graphene; Vibration evenly; Behind ultrasonic dispersion 20min~30min; Stir with constant temperature magnetic force heating stirrer; Speed by 20/min~30 droplet/min when stirring dropwise adds the ammoniacal liquor that concentration is 0.3mol/L~5mol/L, until obtaining water white Graphene-butter of tin colloidal sol;
(3) preparation of particle electrode catalyst filling: with in the step (1) after Graphene-butter of tin colloidal sol described in pretreated aluminium oxide particles electrode and the step (2) mixes by 3: 1~12 mass ratio; Stir with constant temperature magnetic force heating stirrer; Centrifugalize with centrifuge behind still aging then 10h~18h; The solid that centrifugation is obtained is to dry under 80 ℃~90 ℃ the condition in temperature; Solid after will drying again places Muffle furnace, is roasting 2h~4h under 400 ℃~600 ℃ the condition in temperature, obtains the particle electrode catalyst filling of three-diemsnional electrode with the stove cooling.
2. the particle electrode catalyst filling of a kind of three-diemsnional electrode according to claim 1 is characterized in that, the mass concentration of butter of tin solution is 20% described in the step (2).
3. the particle electrode catalyst filling of a kind of three-diemsnional electrode according to claim 1 is characterized in that, the concentration of ammoniacal liquor is 0.4mol/L described in the step (2).
4. the particle electrode catalyst filling of a kind of three-diemsnional electrode according to claim 1 is characterized in that, roasting time is 2h described in the step (3).
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